US20240010496A1 - Atmospheric plasma reactor for the large-scale production of carbon nanotubes and amorphous carbon - Google Patents

Atmospheric plasma reactor for the large-scale production of carbon nanotubes and amorphous carbon Download PDF

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Publication number
US20240010496A1
US20240010496A1 US18/042,021 US202118042021A US2024010496A1 US 20240010496 A1 US20240010496 A1 US 20240010496A1 US 202118042021 A US202118042021 A US 202118042021A US 2024010496 A1 US2024010496 A1 US 2024010496A1
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carbon
plasma
cathode
gas
reactor according
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Aurelio Reis Da Costa Labanca
Cláudio Fernandes Da Silva
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Servico Nacional De Aprendizagem Industrial Senai Dr/rn
Petroleo Brasileiro SA Petrobras
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Servico Nacional De Aprendizagem Industrial Senai Dr/rn
Petroleo Brasileiro SA Petrobras
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Assigned to Servico Nacional de Aprendizagem Industrial - SENAI - DR/RN reassignment Servico Nacional de Aprendizagem Industrial - SENAI - DR/RN ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: FERNANDES DA SILVA, Cláudio
Assigned to Petróleo Brasileiro S.A. - Petrobras reassignment Petróleo Brasileiro S.A. - Petrobras ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: REIS DA COSTA LABANCA, Aurelio
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/16—Preparation
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00—Generating plasma; Handling plasma
    • H05H1/24—Generating plasma
    • H05H1/26—Plasma torches
    • H05H1/32—Plasma torches using an arc
    • H05H1/34—Details, e.g. electrodes, nozzles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/22—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds
    • C01B3/24—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0809—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes employing two or more electrodes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0824—Details relating to the shape of the electrodes
    • B01J2219/0826—Details relating to the shape of the electrodes essentially linear
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0824—Details relating to the shape of the electrodes
    • B01J2219/0826—Details relating to the shape of the electrodes essentially linear
    • B01J2219/083—Details relating to the shape of the electrodes essentially linear cylindrical
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0837—Details relating to the material of the electrodes
    • B01J2219/0841—Metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0871—Heating or cooling of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0875—Gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0892—Materials to be treated involving catalytically active material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0894—Processes carried out in the presence of a plasma
    • B01J2219/0898—Hot plasma
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/13—Nanotubes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H2245/00—Applications of plasma devices
    • H05H2245/50—Production of nanostructures

Definitions

  • the present invention addresses to a plasma reactor with application in the area of thermal decomposition of (light) hydrocarbon molecules, aiming at the production of carbon nanotubes on a large scale, as well as amorphous carbon of superior quality in terms of purity.
  • the hydrogen production process is classified according to the reactions involved in the production of the gas.
  • the material produced by the partial combustion of the load does not have a purity level as high as that of the invention, which performs the pyrolysis of the hydrocarbon using thermal plasma or the heat therefrom.
  • Plasma pyrolysis of hydrocarbons in addition to generating two products (hydrogen and carbon), is an alternative for decarbonizing fossil fuels.
  • the objective is to evaluate its potential in reducing the emission of greenhouse gases.
  • Plasma decarbonization can help in the development of cleaner processes in the carbon production industry, in hydrogen generation or even in electrical generation.
  • Carbon black as it is commercially known, has high added value and great worldwide demand; in addition, plasma pyrolysis of light hydrocarbons, such as methane, provides superior quality carbonaceous materials that are unavailable in the current carbon black market.
  • the molecular breakdown of a hydrocarbon is thermally performed.
  • methane pyrolysis processes that are used in the production of carbon black; in these, the energy needed to break down the CH 4 molecules is provided by the burning of methane itself.
  • An innovative alternative is the breakdown of molecules via plasma, capable of causing the decomposition of methane gas without burning the gas.
  • the generation of electrical discharges inside a reactor under appropriate conditions enables the formation of a plasma arc, which provides thermal energy for the decomposition of the hydrocarbon and adds a catalytic effect to the reaction due to the occurrence of collision processes between the present particles.
  • Document PI0305309-1 discloses a plasma pyrolysis process aiming at producing gaseous hydrogen and solid carbonaceous material from the decomposition of hydrocarbons and alcohols, exemplified here for the decomposition of methane gas and its use.
  • the process consists of supplying thermal energy to the hydrocarbon flow in sufficient quantity for its decomposition reaction.
  • a flow of hydrogen gas is used, which is ionized (the plasma gas) and serves as a vehicle for the decomposition of the hydrocarbon.
  • This flow is initially derived from an external source of hydrogen and subsequently composed of hydrogen generated by the hydrocarbon pyrolysis process itself.
  • a source of direct current electrical energy provides the necessary energy for electrical discharges inside the reactor, in a region called plasma arc.
  • the document discloses a process and method that use plasma for the decomposition of hydrocarbon (methane gas), producing carbon material; however, the invention uses argon gas as plasma gas and, with electric currents on the order of 5 at 20% of that used in the document (PI0305309-1), it is possible to obtain the same test conditions inside the chamber in the present invention. This is due to the different way of injecting the process gases, and also to the new design of the electrodes. The useful life of the electrodes of the present invention is longer, due to the electrical contact of the arc (root of the arc) in the cathode occurring entirely on the surface of the piece of tungsten with 2% thoria.
  • the electrodes of the present invention are made of different materials, are more resistant and present geometric differences. Furthermore, the present invention makes use of different plasma gas, aiming at the production of carbon nanomaterials.
  • the present invention addresses to a plasma reactor aiming at the production of large-scale carbon nanotubes and amorphous carbon, different from what is disclosed by documents of the state of the art.
  • the present invention addresses to a plasma reactor for the thermal decomposition of light hydrocarbon molecules aiming at the production of large-scale carbon nanotubes, as well as amorphous carbon of superior quality in terms of purity. Because it is obtained at pressures close to the atmospheric pressure, said reactor has a superior capacity for the production of nanotubes compared to methods that operate at low pressure.
  • the pyrolysis of hydrocarbons by means of thermal plasma or the heat derived therefrom presents a carbonaceous material with a higher purity content than those obtained by the methods most used in the production of solid carbon (Carbon Black), which are based in the burning of part of the hydrocarbon in the load.
  • Carbon Black solid carbon
  • Yet another objective of the present invention is to provide an alternative for the decarbonization of fossil fuels.
  • Additional objectives of the present invention are related to the reduction of difficulties in assembly and disassembly of the torch, elimination of leaks in the cooling system, elimination of the problem of low thermal dissipation due to the large size of the anode that made its cooling difficult, among others that will be apparent to those skilled on the subject.
  • FIG. 1 illustrating the reaction chamber
  • FIG. 2 illustrating the fastening structure of the plasma pyrolysis equipment
  • FIG. 3 illustrating the plasma torch
  • FIG. 4 illustrating an electrode (cathode
  • FIG. 5 illustrating the torch anodes in the straight (D1), conical (D2) and step (D3) shape
  • FIG. 6 with SEM images of produced carbon nanotubes (E).
  • the plasma reactor (T+C) for the thermal decomposition of hydrocarbon molecules aiming at the production of carbon nanotubes (E) on a large scale and amorphous carbon of superior quality in terms of purity, has a reaction chamber (C) made of stainless steel, as shown in FIG. 1 .
  • the chamber (C) consists of two sections, called the upper section (A) and the lower section (B).
  • the fastening structure of the plasma pyrolysis equipment ( FIG. 2 ) was built in carbon steel. Its base was designed to ensure the stability of the structure, preventing it from toppling over with the weight of the electrode set ( FIG. 3 ) and the reaction chamber (C). The base also has enough space to accommodate the electrical source and the thermostatic bath for cooling the electrodes.
  • the upper section (A) of the reaction chamber (C) has a window to enable the visualization of the electric arc and visual monitoring of the process throughout the reaction tests.
  • the lower section of the chamber (B) consists of only of a temperature sensor input (i) and two larger diameter inputs (ii, iii) that can be used for “QUENCHING”, if necessary, or input for a pressure sensor or even temperature sensor.
  • the upper flange (F) was designed to ensure the coupling of the electrode system for generating the plasma torch (T).
  • This section of the chamber (A) also contains two inputs for temperature sensors (I, II), equidistant from each other, and a third input with a larger diameter that can be used for “QUENCHING” (III) or for inserting a sensor for measuring the temperature at the boundary point between the two sections or even for monitoring the pressure downstream the reaction zone.
  • the plasma torch (T) is provided with an induced magnetic field, responsible for rotating the arc at a predetermined speed, which is an important factor to ensure a homogeneous temperature for the plasma gas at a low consumption of the electrode.
  • the plasma torch (T) supplies the energy necessary for the breakdown of the hydrocarbon load.
  • the radiation therefrom, as well as the heat convection from the plasma gas, provides enough energy for the hydrocarbons in the load to reach the complete pyrolysis temperature of methane molecules (1000° C.).
  • the process should preferably take place at temperatures above 2500° C.
  • FIG. 3 plasma torch
  • the injector ( 1 ) injects the gas in the axial direction.
  • FIG. 4 represents a cathode ( 19 ) and FIG. 5 the anodes (D1, D2, and D3), which, because they are metallic and due to the electrical contact of the cathode arc occur entirely in the piece of tungsten with 2% thoria, the electrodes have a service life at least three times longer than conventional carbon electrodes (U.S. Pat. No. 5,997,837) or another pair of metallic electrodes (PI0305309-1), even with temperatures inside the chamber at the same magnitude.
  • the new torch (T) features a superior design in terms of coupling between parts, more refined, where some parts are coupled through threads; the insert of tungsten with 2% thoria with forced adjustment in a copper piece forming what can be called a cathode ( 19 ), in addition to well-adjusted skirts for safe cooling of the electrodes.
  • the new torch (T) also presents an improved design of the electrodes, which have a longer service life due to the precise thoriated tungsten insert in the cathode ( 19 ) (which forces the root of the electric arc to be located on the external surface of the insert of tungsten with 2% thoria, which works as a cathode—19) and new geometries for three different types of anode.
  • the reaction chamber (C) was tested with the new plasma torch (T), obtaining temperatures inside the chamber (C) in the same magnitude, despite a lower energy consumption compared to PI0305309-1, and producing carbon in solid state.
  • Part of the electrical-electronic system will be installed in the support column ( FIG. 2 -CL) and in the upper cabin ( FIG. 2 -CA), which, in addition to the structural function, will serve as a cabin for passing power cables and installation of electronic components.
  • the upper cabin (CA) will be used to support the set of electrodes and to install pressure and temperature indicators, mass flow controllers, switches in general, starting buttons, stopping the electrical source and control device of the current provided to the system.
  • the carbonaceous material to be obtained may have a high content of carbon nanostructures, such as carbon nanotubes (E), depending mainly on the temperature in the bed zone containing catalysts. It is possible to manufacture carbon nanotubes (E), when catalysts are used inside the reaction chamber (C), and to manufacture amorphous carbon, when catalysts are not used.
  • Argon gas was used as plasma gas, being maintained at an electrical discharge of about 5 to 50 A and 22 to 32 V.
  • the cathode ( 19 ) was cooled with water at a temperature of about 22 to 26° C.
  • helium gas can be used as plasma gas.
  • the heat from the plasma arc is low in the radial direction and the highest temperatures are possible in the region (A) of the chamber (C) downstream of the plasma arc, preferably in the axial axis of the chamber (C). Therefore, the thermal decomposition of methane will occur mainly due to the heat from the plasma torch (T) in the axial direction.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Toxicology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Plasma & Fusion (AREA)
  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Plasma Technology (AREA)
US18/042,021 2020-08-20 2021-08-17 Atmospheric plasma reactor for the large-scale production of carbon nanotubes and amorphous carbon Pending US20240010496A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
BR1020200170341 2020-08-20
BR102020017034-1A BR102020017034A2 (pt) 2020-08-20 2020-08-20 Reator atmosférico a plasma para produção de nanotubos de carbono em larga escala e carbono amorfo
PCT/BR2021/050347 WO2022036428A1 (pt) 2020-08-20 2021-08-17 Reator atmosférico a plasma para produção de nanotubos de carbono em larga escala e carbono amorfo

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US (1) US20240010496A1 (pt)
JP (1) JP2023538103A (pt)
CN (1) CN116349412A (pt)
BR (1) BR102020017034A2 (pt)
CA (1) CA3189872A1 (pt)
DE (1) DE112021004387T5 (pt)
WO (1) WO2022036428A1 (pt)

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NO175718C (no) * 1991-12-12 1994-11-23 Kvaerner Eng Fremgangsmåte ved spalting av hydrokarboner samt apparat for bruk ved fremgangsmåten
NO176522C (no) * 1992-04-07 1995-04-19 Kvaerner Eng Fremgangsmåte ved fremstilling av karbon med definerte fysikalske egenskaper samt apparat for gjennomföring av fremgangsmåten
FR2813158A1 (fr) * 2000-08-18 2002-02-22 Air Liquide Electrode pour torche a plasma a insert emissif de duree de vie amelioree
US20130039838A1 (en) * 2007-06-15 2013-02-14 Nanocomp Technologies, Inc. Systems and methods for production of nanostructures using a plasma generator
CN108675282A (zh) * 2018-04-19 2018-10-19 华北电力大学 等离子体加强火焰法制备碳纳米管工业量产装置
KR102228888B1 (ko) * 2019-01-21 2021-03-17 엘지전자 주식회사 열플라즈마 처리장치

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JP2023538103A (ja) 2023-09-06
BR102020017034A2 (pt) 2022-03-03
CN116349412A (zh) 2023-06-27
CA3189872A1 (en) 2022-02-24
DE112021004387T5 (de) 2023-06-01

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